Ammonia → HCID 89826370, compound

Participants

Reaction Conditions

Reaction Steps

To a suspension of 143 mg (0.5 mmol) 7-fluoro-3-[4-(1-hydroxy-1-methyl-ethyl)-phenyl]-2H-pyrrolo[1,2-a]pyrazin-1-one and 71.5 mg (1.1 mmol) sodium azide in 1 ml dichloromethane is added dropwise under external cooling with ice a solution of 316 μl (4.1 mmol) trifluoroacetic acid in 0.6 ml dichloromethane. The reaction mixture is stirred for 3 hours at 0° C. Ice and 25% aqueous ammonia are added to obtain a two-phase mixture with a pH of 11. Then a 1:1 mixture of cyclohexane/ethyl acetate is added. The organic phase is separated, dried over sodium sulfate and evaporated to afford 3-[4-(1-azido-1-methyl-ethyl)-phenyl]-7-fluoro-2H-pyrrolo[1,2-a]pyrazin-1-one as beige powder; HPLC/MS 2.29 min (A), [M+H] 312.

Provenance & Evidence